CN103539086B - A kind of processing method preparing non-polar surface aluminum nitride material - Google Patents
A kind of processing method preparing non-polar surface aluminum nitride material Download PDFInfo
- Publication number
- CN103539086B CN103539086B CN201210258779.8A CN201210258779A CN103539086B CN 103539086 B CN103539086 B CN 103539086B CN 201210258779 A CN201210258779 A CN 201210258779A CN 103539086 B CN103539086 B CN 103539086B
- Authority
- CN
- China
- Prior art keywords
- temperature
- crucible
- aluminum nitride
- nitride material
- aluminium nitride
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The invention belongs to field of material preparation, it is provided that a kind of processing method preparing non-polar surface aluminum nitride material, mainly through the temperature head of crucible top and crucible body in control growth temperature and growing apparatus, it is achieved the preparation of high quality non-polar surface aluminum nitride material. Concrete preparation process comprises: aluminium nitride material is carried out high temperature sintering pre-treatment by (1) material pre-treatment in nitrogen atmosphere; (2) temperature rise period is in nitrogen atmosphere, does aluminum nitride source with pretreated material, heats up by certain speed, and keeps crucible top and crucible body to have certain temperature head; (3) after holding stage is warming up to suitable growth temperature, the temperature head between adjustment crucible top and crucible body, enters holding stage, prepares aluminium nitride by material distillation; (4) after temperature-fall period is incubated for some time, again adjusting the temperature head between crucible top and crucible body, then start to reduce temperature to room temperature, growth terminates.
Description
Technical field
The invention belongs to field of material preparation, in particular to a kind of processing method preparing non-polar surface aluminum nitride material.
Background technology
Aluminium nitride (AlN), as a kind of novel semiconductor material, has energy gap big (6.2eV), thermal conductivity height (3.4W cm-1·K-1), breakdown field powerful (1.8 × 106V·cm-1), chemistry and the advantage such as Heat stability is good, be the ideal material making short wavelength's ultraviolet light emitting device, ultraviolet detector and high temperature high power microwave electronic device, photoelectron and microelectronic can be widely used in. The research of aluminium nitride material and device is all carry out on the c plane materiel material of relatively easily growth by restriction at present substantially that be subject to technology of preparing. Due to the impact that the wurtzite structure of aluminium nitride material and the electronegativity of Al atom and atom N differ greatly, aluminium nitride and heterojunction thereof is caused to have very strong piezoelectricity and spontaneous polarization effect at c direction of principal axis. Polarizing effect produces the built in field of high strength in the aluminum nitride epitaxial layer grown along c direction of principal axis. The existence of this built in field causes quantum limit STARK effect, band curvature and level of energy is changed, thus causes emission wavelength generation red shift, and electronics and hole wave function crossover diminish and cause quantum well luminous efficiency to decline simultaneously. In order to eliminate polarizing effect to the impact of device light emitting efficiency, most basic method is aluminium nitride material and the heterojunction structure thereof of growing nonpolar face. Due to existing technology of preparing and find and suppress not overcome the effective ways of the stronger anisotropic growth characteristic of aluminium nitride material (aluminium nitride is obvious along c direction of principal axis preferential growth trend), current growing high-quality, non-polar surface aluminum nitride material have become the difficult point of wide bandgap semiconductor field research.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, in conjunction with the feature of aluminium nitride material self, a kind of processing method preparing non-polar surface aluminum nitride material is provided, this processing method, by the temperature head of crucible top and crucible body in control growing apparatus, realizes the preparation of high quality non-polar surface aluminum nitride material.
The enforcement of the present invention comprises:
(1) material pre-treatment is in nitrogen atmosphere, and aluminium nitride material is carried out high temperature sintering pre-treatment, reduces the possibility introducing the impurity such as oxygen by material in aluminium nitride as much as possible;
(2) temperature rise period taking through high temperature pretreated material as aluminum nitride source, in the nitrogen atmosphere of 0.1～5 normal atmosphere, heat up by certain speed, and keeping the Temperature Ratio crucible height 20～150 DEG C on crucible top, the nucleus that the Developing restraint initial stage is too much and aluminium nitride are along the crystallization of c direction of principal axis;
(3) after holding stage is warming up to the growth temperature of 2250～2350 DEG C, temperature head between adjustment crucible top and crucible body, make Temperature Ratio crucible body low 10～200 DEG C on crucible top, impel the growth of non-polar plane, then enter holding stage, prepare non-polar plane aluminium nitride by material distillation;
(4), after temperature-fall period is incubated for some time, again adjusts the temperature head between crucible top and crucible body, make the Temperature Ratio crucible height 20～150 DEG C on crucible top, the secondary crystal at aln surface in Developing restraint later stage, then starting cooling, after temperature is down to room temperature, growth terminates.
Accompanying drawing explanation
Fig. 1 is the diagrammatic cross-section being used growing apparatus in the embodiment of the present invention 1
Fig. 2 is the diagrammatic cross-section being used growing apparatus in the embodiment of the present invention 2
Embodiment
The present invention provides a kind of processing method preparing non-polar surface aluminum nitride material. Prepare the embodiment of nonpolar aluminium nitride material below with the present invention for two, the present invention will be further described.
Embodiment 1:
This embodiment uses the growing apparatus of Frequency Induction Heating, as shown in Figure 1. This device comprises top thermo detector (1), load coil (2), lagging material (3), tungsten crucible (4), aluminium nitride material (5), side thermo detector (6), crucible lifting system (7).
First, using aluminium nitride polycrystalline as material, and the high temperature pre-treatment before it is grown in nitrogen environment, to reduce the possibility introducing the impurity such as oxygen by material in aluminium nitride as much as possible. Then, do aluminum nitride source with material after pre-treatment, in the nitrogen environment of 1 normal atmosphere and the growth temperature of 2300 DEG C carry out aluminium nitride growth experiment. Process of growth comprises three phases: (a) temperature rise period heats up with the speed of 300 DEG C/h, in temperature-rise period, by the upper-lower position of crucible lifting system call interception tungsten crucible in load coil, meet crucible top higher than the temperature of crucible body 80 DEG C, to suppress the nuclei of crystallization too much at the crystallization initial stage on crucible cover and the growth along c direction of principal axis; B () holding stage temperature adjusts the upper-lower position of tungsten crucible after rising to 2300 DEG C again, ensure that crucible top is lower than the temperature of crucible body 50 DEG C, to realize the growth of aluminium nitride on crucible top substrate; C () temperature-fall period is after the soaking time of 8 hours, again adjust the upper-lower position of tungsten crucible, meet crucible top higher than the temperature of crucible body 80 DEG C, the secondary crystal at aln surface in Developing restraint later stage, then cooling is started, after temperature is down to room temperature, experiment completes, and prepares non-pole profile aluminium nitride material.
Embodiment 2:
This embodiment uses the growing apparatus of two resistance heater, as shown in Figure 2, this device comprises: top thermo detector (1), lagging material (2), top heater (3), side heater (4), tungsten crucible (5), aluminium nitride material (6), side thermo detector (7).
The step of this embodiment is basic identical with embodiment 1, institute the difference is that: in (i) the present embodiment, the mode of employing resistive heating; (ii), in the present embodiment, guarantee between crucible top and crucible body, to meet suitable temperature head condition by the mode of adjustment top heater and side heater heating power.
Claims (1)
1. prepare a processing method for non-polar surface aluminum nitride material, comprise the steps: that aluminium nitride material is carried out high temperature sintering pre-treatment by (1) in nitrogen atmosphere; (2) in nitrogen atmosphere, it may also be useful to do aluminum nitride source through pretreated aluminium nitride material, heat up by certain speed, and the Temperature Ratio crucible height 20～150 DEG C on crucible top is kept; (3) after being warming up to the growth temperature of 2250～2350 DEG C, the temperature head between adjustment crucible top and crucible body, makes Temperature Ratio crucible body low 10～200 DEG C on crucible top, enters holding stage, prepares aluminium nitride by material distillation; (4) after being incubated for some time, again adjusting the temperature head between crucible top and crucible body, make the Temperature Ratio crucible height 20～150 DEG C on crucible top, then start to reduce temperature to room temperature, growth terminates.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210258779.8A CN103539086B (en) | 2012-07-17 | 2012-07-17 | A kind of processing method preparing non-polar surface aluminum nitride material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210258779.8A CN103539086B (en) | 2012-07-17 | 2012-07-17 | A kind of processing method preparing non-polar surface aluminum nitride material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103539086A CN103539086A (en) | 2014-01-29 |
| CN103539086B true CN103539086B (en) | 2016-06-15 |
Family
ID=49963010
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210258779.8A Active CN103539086B (en) | 2012-07-17 | 2012-07-17 | A kind of processing method preparing non-polar surface aluminum nitride material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103539086B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106149057A (en) * | 2015-03-10 | 2016-11-23 | 深圳大学 | The controlled aluminum nitride crystal growth device in temperature field and technique |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101050545A (en) * | 2006-04-03 | 2007-10-10 | 深圳大学 | Method for developing aluminum nitride crystal in large size through flow of plasma flame |
| CN101070618A (en) * | 2007-03-19 | 2007-11-14 | 宁波工程学院 | Monocrystal AIN nano chain |
| CN101798072A (en) * | 2010-04-23 | 2010-08-11 | 中南大学 | Method for preparing ultra-fine aluminum nitride powder |
-
2012
- 2012-07-17 CN CN201210258779.8A patent/CN103539086B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101050545A (en) * | 2006-04-03 | 2007-10-10 | 深圳大学 | Method for developing aluminum nitride crystal in large size through flow of plasma flame |
| CN101070618A (en) * | 2007-03-19 | 2007-11-14 | 宁波工程学院 | Monocrystal AIN nano chain |
| CN101798072A (en) * | 2010-04-23 | 2010-08-11 | 中南大学 | Method for preparing ultra-fine aluminum nitride powder |
Non-Patent Citations (1)
| Title |
|---|
| 气相生长氮化铝单晶的新方法;武红磊等;《人工晶体学报》;20070228;第36卷(第01期);1-4 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103539086A (en) | 2014-01-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US9340898B2 (en) | Process for growing silicon carbide single crystal by physical vapor transport method and annealing silicon carbide single crystal in situ | |
| CN107904657A (en) | A kind of growing method of PVT methods growing large-size Semi-insulating silicon carbide mono-crystal | |
| CN106757357B (en) | A kind of preparation method of high-purity semi-insulating silicon carbide substrate | |
| US20120118228A1 (en) | Sapphire ingot grower | |
| JP2014133701A (en) | One hundred millimeter high purity semi-insulating single crystal silicon carbide wafer | |
| CN101724906B (en) | Method for growing high-quality conductive silicon carbide crystal | |
| CN104947182A (en) | Method for rapidly growing large-size high-purity semi-insulating silicon carbide single crystal | |
| CN102828239B (en) | Method for preparing self-supporting substrate from gallium nitride single-crystal materials by self-separating by aid of defect and stress removal technology | |
| CN103060904B (en) | A kind of method being realized AlN single crystal growing by growth pattern regulation and control | |
| CN101724893A (en) | Method for preparing high-purity semi-insulating silicon carbide crystalloid | |
| CN103199008A (en) | Homoepitaxial method on zero offset 4H-SiC substrate | |
| CN103305903B (en) | A kind of high nitrogen pressure fusing assistant-falling crucible method prepares the method for GaN crystal | |
| CN101597790B (en) | Method for preparing cast polycrystalline silicon through melting silicon and doping nitrogen under nitrogen | |
| CN103103611A (en) | Device and process for preparing aluminum nitride crystals by adopting spontaneous crystal seed method | |
| CN107460541A (en) | The aluminum nitride crystal growth device controllable for raw material distillation and application method | |
| CN107557872A (en) | A kind of large size silicon carbide crystals situ heat treatment method | |
| CN104779141A (en) | Preparation method of low-deflection angle silicon carbide homogeneous epitaxial material | |
| CN103539086B (en) | A kind of processing method preparing non-polar surface aluminum nitride material | |
| CN207608656U (en) | A kind of grower of PVT methods growing large-size Semi-insulating silicon carbide mono-crystal | |
| CN103060902B (en) | Direct forming prepares method and the silicon chip direct-forming device of band silicon | |
| CN106801258A (en) | A kind of preparation method with hexa-prism aluminium nitride whisker | |
| CN105006427B (en) | A kind of method that high-quality gallium nitride epitaxial structure is grown using low temperature buffer layer | |
| CN108286074B (en) | Large-size SiC single crystal growth device and working method thereof | |
| CN218175203U (en) | Eight-inch PVT growth furnace with adjustable thermal field | |
| CN108330536B (en) | Preparation method of PA-MBE homoepitaxy high-quality GaN monocrystal film |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |